Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 186 _publ_contact_author_name 'Dr Leone Spiccia' _publ_contact_author_address ; School of Chemistry Monash University PO Box 23 Clayton Victoria 3800 AUSTRALIA ; _publ_contact_author_fax ' +61 3 9905 4597 ' _publ_contact_author_phone ' +61 3 9905 4526 ' _publ_contact_author_email ' leone.spiccia@sci.monash.edu.au ' _publ_requested_journal 'Dalton Transactions' _publ_requested_category ? _publ_section_title ; Asymmetry in Endogenously Bridged Binuclear Copper(II) and Zinc(II) Complexes Formed by 1,2-bis[1,4,7-triazacyclonon-1-yl] propan-2-ol ; loop_ _publ_author_name _publ_author_address 'Fry, F. H.' ; School of Chemistry PO Box 23 Monash University 3800 Australia ; 'Moubaraki, B.' ; School of Chemistry PO Box 23 Monash University 3800 Australia ; 'Murray, K. S.' ; School of Chemistry PO Box 23 Monash University 3800 Australia ; 'Spiccia, L.' ; School of Chemistry PO Box 23 Monash University 3800 Australia ; 'Warren, M.' ; School of Chemistry PO Box 23 Monash University 3800 Australia ; 'Skelton, B. W.' ; Department of Chemistry University of Western Australia 35 Stirling Highway Crawley Western Australia 6009 Australia ; 'White, A. H.' ; Department of Chemistry University of Western Australia 35 Stirling Highway Crawley Western Australia 6009 Australia ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_1 _database_code_CSD 198150 _audit_creation_method Xtal3.6 _audit_creation_date 99-10-12 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C15 H33 Br3 Cu2 N6 O3' _chemical_formula_moiety [Cu2(T2PrO)Br2]Br.2H2O _chemical_formula_weight 712.27 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 7.4380(10) _cell_length_b 13.326(2) _cell_length_c 13.812(3) _cell_angle_alpha 64.635(2) _cell_angle_beta 78.858(3) _cell_angle_gamma 89.469(3) _cell_volume 1209.6(4) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.967 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 4333 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 6.74 _exptl_crystal_description bar _exptl_crystal_size_max .55 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .16 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .371 _exptl_absorpt_correction_T_max .894 _diffrn_reflns_number 13565 _reflns_number_total 5844 _reflns_Friedel_coverage ? _reflns_number_gt 4201 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.13 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .0683 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .054 _refine_ls_wR_factor_ref .061 _refine_ls_goodness_of_fit_ref 1.802 _refine_ls_number_reflns 4201 _refine_ls_number_parameters 272 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .043 _refine_diff_density_min -1.22 _refine_diff_density_max 1.813 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 30 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 74 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Br ? 0 6 -.374 2.456 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 4 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 12 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 6 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 .85636(9) .29522(6) -.13398(6) .0286(6) Uani ? ? 1.00000 ? ? Cu2 .75972(10) .17300(6) .15941(6) .0341(7) Uani ? ? 1.00000 ? ? Br0 1.92329(13) .23986(7) .51297(7) .0656(9) Uani ? ? 1.00000 ? ? Br1 .61530(9) .15272(5) -.09220(6) .0392(6) Uani ? ? 1.00000 ? ? Br2 .56180(9) .32500(6) .13197(7) .0480(7) Uani ? ? 1.00000 ? ? C11 1.2000(9) .3322(6) -.0869(6) .048(7) Uani ? ? 1.00000 ? ? N11 1.1066(6) .3893(4) -.1782(4) .035(5) Uani ? ? 1.00000 ? ? C12 1.1988(9) .3843(6) -.2810(6) .045(7) Uani ? ? 1.00000 ? ? C13 1.0642(9) .4128(6) -.3584(6) .045(7) Uani ? ? 1.00000 ? ? N14 .8809(7) .3534(4) -.2972(4) .036(5) Uani ? ? 1.00000 ? ? C15 .7236(9) .4228(6) -.3244(6) .046(7) Uani ? ? 1.00000 ? ? C16 .7137(10) .5068(6) -.2768(6) .051(7) Uani ? ? 1.00000 ? ? N17 .7383(7) .4546(4) -.1625(5) .039(5) Uani ? ? 1.00000 ? ? C18 .8794(11) .5124(6) -.1395(7) .053(8) Uani ? ? 1.00000 ? ? C19 1.0717(10) .5051(6) -.1961(6) .048(7) Uani ? ? 1.00000 ? ? C0 1.098(2) .2278(13) .0011(14) .028(13) Uani ? ? .50000 ? ? C0' 1.074(2) .2661(14) .0184(15) .038(15) Uani ? ? .50000 ? ? O0 .9049(5) .2372(3) .0119(3) .034(4) Uani ? ? 1.00000 ? ? C21 1.1533(9) .1814(6) .1064(6) .049(7) Uani ? ? 1.00000 ? ? N21 1.0059(7) .1054(4) .1964(4) .036(5) Uani ? ? 1.00000 ? ? C22 1.0036(9) .1057(7) .3033(6) .052(8) Uani ? ? 1.00000 ? ? C23 .8214(10) .0535(7) .3803(6) .052(7) Uani ? ? 1.00000 ? ? N24 .6690(7) .0981(5) .3235(5) .044(6) Uani ? ? 1.00000 ? ? C25 .5212(10) .0113(8) .3456(6) .064(8) Uani ? ? 1.00000 ? ? C26 .5860(11) -.0606(7) .2886(6) .062(8) Uani ? ? 1.00000 ? ? N27 .6816(8) .0095(5) .1739(4) .046(6) Uani ? ? 1.00000 ? ? C28 .8599(13) -.0265(6) .1429(6) .059(8) Uani ? ? 1.00000 ? ? C29 .9994(10) -.0084(6) .2025(6) .053(7) Uani ? ? 1.00000 ? ? O01 1.5202(13) .3650(8) .4907(8) .148(14) Uani ? ? 1.00000 ? ? O02 1.3645(10) .2188(5) 1.4128(6) .104(9) Uani ? ? 1.00000 ? ? H0 1.13081 .16654 -.01382 .03200 Uiso ? ? .50000 ? ? H0' 1.06556 .33472 .02945 .05300 Uiso ? ? .50000 ? ? H11a 1.27375 .38586 -.08001 .06600 Uiso ? ? 1.00000 ? ? H11b 1.27871 .28136 -.10267 .06600 Uiso ? ? 1.00000 ? ? H12a 1.23688 .30972 -.26393 .05800 Uiso ? ? 1.00000 ? ? H12b 1.30781 .43440 -.31446 .05800 Uiso ? ? 1.00000 ? ? H13a 1.11087 .39173 -.41613 .05800 Uiso ? ? 1.00000 ? ? H13b 1.05389 .49060 -.38905 .05800 Uiso ? ? 1.00000 ? ? H14 .86467 .28993 -.31289 .04700 Uiso ? ? 1.00000 ? ? H15a .60987 .37448 -.29358 .06100 Uiso ? ? 1.00000 ? ? H15b .73537 .45897 -.40158 .06100 Uiso ? ? 1.00000 ? ? H16a .59928 .54052 -.27916 .06500 Uiso ? ? 1.00000 ? ? H16b .81068 .56620 -.31905 .06500 Uiso ? ? 1.00000 ? ? H17 .62060 .44219 -.11416 .04900 Uiso ? ? 1.00000 ? ? H18a .87351 .47951 -.06059 .06600 Uiso ? ? 1.00000 ? ? H18b .85478 .58963 -.16021 .06600 Uiso ? ? 1.00000 ? ? H19a 1.16142 .53429 -.17207 .05900 Uiso ? ? 1.00000 ? ? H19b 1.08381 .55118 -.27401 .05900 Uiso ? ? 1.00000 ? ? H21a 1.26090 .14505 .10355 .06200 Uiso ? ? 1.00000 ? ? H21b 1.18069 .24410 .12346 .06200 Uiso ? ? 1.00000 ? ? H22a 1.02228 .18007 .29358 .06800 Uiso ? ? 1.00000 ? ? H22b 1.10261 .06476 .33306 .06800 Uiso ? ? 1.00000 ? ? H23a .80906 .06630 .44400 .06300 Uiso ? ? 1.00000 ? ? H23b .81656 -.02718 .40501 .06300 Uiso ? ? 1.00000 ? ? H24 .61557 .15040 .34778 .05700 Uiso ? ? 1.00000 ? ? H25a .41554 .04823 .31848 .07900 Uiso ? ? 1.00000 ? ? H25b .48075 -.03332 .42266 .07900 Uiso ? ? 1.00000 ? ? H26a .66573 -.11265 .32794 .08100 Uiso ? ? 1.00000 ? ? H26b .48101 -.10383 .28961 .08100 Uiso ? ? 1.00000 ? ? H27 .59978 .01833 .12564 .05800 Uiso ? ? 1.00000 ? ? H28a .90588 .01531 .06605 .07300 Uiso ? ? 1.00000 ? ? H28b .84620 -.10318 .15985 .07300 Uiso ? ? 1.00000 ? ? H29a 1.11750 -.02185 .17435 .06500 Uiso ? ? 1.00000 ? ? H29b .96413 -.06008 .27951 .06500 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu1 .0264(4) .0286(4) .0264(4) -.0023(3) -.0015(3) -.0094(3) Cu2 .0291(4) .0392(5) .0295(5) .0043(3) .0029(3) -.0145(4) Br0 .0883(7) .0583(5) .0498(5) -.0025(4) -.0057(4) -.0264(4) Br1 .0375(4) .0389(4) .0384(4) -.0098(3) -.0026(3) -.0162(3) Br2 .0391(4) .0509(4) .0602(5) .0142(3) -.0062(3) -.0319(4) C11 .032(3) .056(4) .042(5) -.008(3) -.008(3) -.007(4) N11 .029(3) .032(3) .032(3) -.006(2) .001(2) -.005(2) C12 .038(4) .044(4) .040(4) -.005(3) .011(3) -.014(3) C13 .049(4) .049(4) .033(4) -.010(3) .008(3) -.022(3) N14 .039(3) .039(3) .029(3) -.003(2) -.002(2) -.016(3) C15 .046(4) .054(4) .032(4) .003(3) -.008(3) -.014(3) C16 .052(4) .042(4) .050(5) .014(3) -.011(4) -.012(4) N17 .040(3) .035(3) .038(3) .004(2) -.002(3) -.015(3) C18 .065(5) .036(4) .059(5) .002(4) -.005(4) -.025(4) C19 .051(4) .040(4) .053(5) -.009(3) -.008(4) -.022(4) C0 .019(6) .033(9) .036(9) .002(6) -.000(5) -.022(7) C0' .035(9) .043(11) .033(9) -.002(8) -.007(7) -.014(8) O0 .022(2) .047(3) .024(2) -.0004(19) .0011(17) -.010(2) C21 .028(3) .059(5) .042(5) .005(3) -.003(3) -.009(4) N21 .037(3) .042(3) .024(3) .006(2) -.001(2) -.012(2) C22 .044(4) .073(5) .040(5) -.000(4) -.013(3) -.022(4) C23 .061(5) .076(5) .024(4) -.005(4) -.002(3) -.028(4) N24 .038(3) .061(4) .035(3) .003(3) .005(3) -.028(3) C25 .039(4) .094(6) .040(5) -.015(4) .005(3) -.017(5) C26 .077(6) .065(5) .031(4) -.037(4) .004(4) -.014(4) N27 .063(4) .049(3) .023(3) -.016(3) -.002(3) -.016(3) C28 .100(7) .037(4) .037(5) .002(4) .001(4) -.021(4) C29 .062(5) .044(4) .048(5) .020(4) -.003(4) -.018(4) O01 .127(7) .175(9) .138(9) .023(7) -.057(6) -.050(7) O02 .113(6) .070(4) .100(6) .023(4) .006(4) -.022(4) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu1 Br1 . . 2.4245(10) ? Cu1 N11 . . 2.087(5) ? Cu1 N14 . . 2.015(6) ? Cu1 N17 . . 2.195(6) ? Cu1 O0 . . 1.931(4) ? Cu2 Br2 . . 2.4324(11) ? Cu2 O0 . . 1.930(4) ? Cu2 N21 . . 2.088(5) ? Cu2 N24 . . 2.018(6) ? Cu2 N27 . . 2.175(7) ? C11 N11 . . 1.469(9) ? C11 C0 . . 1.485(14) ? C11 C0' . . 1.471(16) ? C11 H11a . . .952 ? C11 H11b . . .959 ? N11 C12 . . 1.481(10) ? N11 C19 . . 1.484(10) ? C12 C13 . . 1.532(11) ? C12 H12a . . .971 ? C12 H12b . . .958 ? C13 N14 . . 1.484(8) ? C13 H13a . . .959 ? C13 H13b . . .946 ? N14 C15 . . 1.489(9) ? N14 H14 . . .973 ? C15 C16 . . 1.517(13) ? C15 H15a . . .973 ? C15 H15b . . .949 ? C16 N17 . . 1.476(10) ? C16 H16a . . .958 ? C16 H16b . . .969 ? N17 C18 . . 1.466(11) ? N17 H17 . . .960 ? C18 C19 . . 1.515(11) ? C18 H18a . . .977 ? C18 H18b . . .969 ? C19 H19a . . .953 ? C19 H19b . . .970 ? C0 O0 . . 1.424(16) ? C0 C21 . . 1.46(2) ? C0 H0 . . .94 ? C0' O0 . . 1.35(2) ? C0' C21 . . 1.480(18) ? C0' H0' . . .99 ? C21 N21 . . 1.479(7) ? C21 H21a . . .935 ? C21 H21b . . .993 ? N21 C22 . . 1.475(11) ? N21 C29 . . 1.482(11) ? C22 C23 . . 1.510(9) ? C22 H22a . . .949 ? C22 H22b . . .962 ? C23 N24 . . 1.479(10) ? C23 H23a . . .953 ? C23 H23b . . .978 ? N24 C25 . . 1.493(11) ? N24 H24 . . .948 ? C25 C26 . . 1.504(15) ? C25 H25a . . .974 ? C25 H25b . . .957 ? C26 N27 . . 1.482(8) ? C26 H26a . . .961 ? C26 H26b . . .969 ? N27 C28 . . 1.455(11) ? N27 H27 . . .958 ? C28 C29 . . 1.523(14) ? C28 H28a . . .955 ? C28 H28b . . .947 ? C29 H29a . . .938 ? C29 H29b . . .971 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Br1 Cu1 N11 . . . 165.42(17) ? Br1 Cu1 N14 . . . 93.39(16) ? Br1 Cu1 N17 . . . 110.01(15) ? Br1 Cu1 O0 . . . 96.11(12) ? N11 Cu1 N14 . . . 83.7(2) ? N11 Cu1 N17 . . . 83.9(2) ? N11 Cu1 O0 . . . 83.88(19) ? N14 Cu1 N17 . . . 82.8(2) ? N14 Cu1 O0 . . . 164.17(18) ? N17 Cu1 O0 . . . 105.7(2) ? Br2 Cu2 O0 . . . 95.90(13) ? Br2 Cu2 N21 . . . 149.07(18) ? Br2 Cu2 N24 . . . 94.12(18) ? Br2 Cu2 N27 . . . 125.91(17) ? O0 Cu2 N21 . . . 82.42(18) ? O0 Cu2 N24 . . . 165.9(2) ? O0 Cu2 N27 . . . 99.3(2) ? N21 Cu2 N24 . . . 83.9(2) ? N21 Cu2 N27 . . . 84.6(2) ? N24 Cu2 N27 . . . 82.7(3) ? N11 C11 C0 . . . 114.1(9) ? N11 C11 C0' . . . 113.8(9) ? N11 C11 H11a . . . 109.2 ? N11 C11 H11b . . . 109.0 ? C0 C11 H11a . . . 128.3 ? C0 C11 H11b . . . 82.8 ? C0' C11 H11a . . . 109.6 ? C0' C11 H11b . . . 106.6 ? H11a C11 H11b . . . 108.5 ? Cu1 N11 C11 . . . 105.4(3) ? Cu1 N11 C12 . . . 103.7(5) ? Cu1 N11 C19 . . . 109.4(4) ? C11 N11 C12 . . . 113.4(5) ? C11 N11 C19 . . . 112.6(7) ? C12 N11 C19 . . . 111.7(5) ? N11 C12 C13 . . . 109.0(5) ? N11 C12 H12a . . . 109.1 ? N11 C12 H12b . . . 110.4 ? C13 C12 H12a . . . 110.2 ? C13 C12 H12b . . . 111.0 ? H12a C12 H12b . . . 107.1 ? C12 C13 N14 . . . 110.1(5) ? C12 C13 H13a . . . 109.2 ? C12 C13 H13b . . . 108.8 ? N14 C13 H13a . . . 110.1 ? N14 C13 H13b . . . 109.5 ? H13a C13 H13b . . . 109.1 ? Cu1 N14 C13 . . . 111.8(5) ? Cu1 N14 C15 . . . 105.9(4) ? Cu1 N14 H14 . . . 107.8 ? C13 N14 C15 . . . 114.4(5) ? C13 N14 H14 . . . 108.9 ? C15 N14 H14 . . . 107.8 ? N14 C15 C16 . . . 110.7(7) ? N14 C15 H15a . . . 109.0 ? N14 C15 H15b . . . 109.6 ? C16 C15 H15a . . . 108.9 ? C16 C15 H15b . . . 111.0 ? H15a C15 H15b . . . 107.6 ? C15 C16 N17 . . . 111.2(6) ? C15 C16 H16a . . . 111.7 ? C15 C16 H16b . . . 109.9 ? N17 C16 H16a . . . 109.0 ? N17 C16 H16b . . . 107.7 ? H16a C16 H16b . . . 107.2 ? Cu1 N17 C16 . . . 107.6(5) ? Cu1 N17 C18 . . . 101.3(4) ? Cu1 N17 H17 . . . 110.2 ? C16 N17 C18 . . . 114.8(5) ? C16 N17 H17 . . . 108.9 ? C18 N17 H17 . . . 113.6 ? N17 C18 C19 . . . 112.4(8) ? N17 C18 H18a . . . 109.4 ? N17 C18 H18b . . . 110.4 ? C19 C18 H18a . . . 108.5 ? C19 C18 H18b . . . 110.3 ? H18a C18 H18b . . . 105.7 ? N11 C19 C18 . . . 112.0(5) ? N11 C19 H19a . . . 110.0 ? N11 C19 H19b . . . 108.8 ? C18 C19 H19a . . . 110.6 ? C18 C19 H19b . . . 107.7 ? H19a C19 H19b . . . 107.6 ? C11 C0 O0 . . . 110.2(10) ? C11 C0 C21 . . . 117.8(14) ? C11 C0 H0 . . . 110.3 ? O0 C0 C21 . . . 112.6(11) ? O0 C0 H0 . . . 110.6 ? C21 C0 H0 . . . 94.2 ? C11 C0' C21 . . . 117.3(12) ? C11 C0' H0' . . . 87.4 ? O0 C0' C21 . . . 115.8(11) ? O0 C0' H0' . . . 107.2 ? C21 C0' H0' . . . 108.8 ? Cu1 O0 Cu2 . . . 136.2(2) ? Cu1 O0 C0 . . . 106.8(8) ? Cu1 O0 C0' . . . 115.7(8) ? Cu2 O0 C0 . . . 116.2(7) ? Cu2 O0 C0' . . . 106.5(8) ? C0 C21 N21 . . . 112.2(8) ? C0 C21 H21a . . . 111.4 ? C0 C21 H21b . . . 108.0 ? C0' C21 N21 . . . 110.5(8) ? C0' C21 H21a . . . 131.2 ? C0' C21 H21b . . . 84.6 ? N21 C21 H21a . . . 110.3 ? N21 C21 H21b . . . 107.7 ? H21a C21 H21b . . . 107.2 ? Cu2 N21 C21 . . . 105.8(4) ? Cu2 N21 C22 . . . 102.6(4) ? Cu2 N21 C29 . . . 108.0(5) ? C21 N21 C22 . . . 114.2(6) ? C21 N21 C29 . . . 112.4(6) ? C22 N21 C29 . . . 112.9(5) ? N21 C22 C23 . . . 110.0(7) ? N21 C22 H22a . . . 109.6 ? N21 C22 H22b . . . 108.8 ? C23 C22 H22a . . . 109.5 ? C23 C22 H22b . . . 110.4 ? H22a C22 H22b . . . 108.5 ? C22 C23 N24 . . . 110.1(5) ? C22 C23 H23a . . . 110.6 ? C22 C23 H23b . . . 109.2 ? N24 C23 H23a . . . 110.7 ? N24 C23 H23b . . . 109.2 ? H23a C23 H23b . . . 106.9 ? Cu2 N24 C23 . . . 111.2(4) ? Cu2 N24 C25 . . . 106.0(5) ? Cu2 N24 H24 . . . 109.8 ? C23 N24 C25 . . . 113.8(6) ? C23 N24 H24 . . . 107.8 ? C25 N24 H24 . . . 108.1 ? N24 C25 C26 . . . 111.0(6) ? N24 C25 H25a . . . 108.8 ? N24 C25 H25b . . . 110.6 ? C26 C25 H25a . . . 108.9 ? C26 C25 H25b . . . 110.5 ? H25a C25 H25b . . . 106.9 ? C25 C26 N27 . . . 110.3(6) ? C25 C26 H26a . . . 109.6 ? C25 C26 H26b . . . 109.1 ? N27 C26 H26a . . . 110.8 ? N27 C26 H26b . . . 109.9 ? H26a C26 H26b . . . 107.1 ? Cu2 N27 C26 . . . 108.5(6) ? Cu2 N27 C28 . . . 101.3(5) ? Cu2 N27 H27 . . . 108.4 ? C26 N27 C28 . . . 113.8(5) ? C26 N27 H27 . . . 109.6 ? C28 N27 H27 . . . 114.6 ? N27 C28 C29 . . . 111.7(8) ? N27 C28 H28a . . . 109.4 ? N27 C28 H28b . . . 109.1 ? C29 C28 H28a . . . 108.1 ? C29 C28 H28b . . . 109.3 ? H28a C28 H28b . . . 109.3 ? N21 C29 C28 . . . 112.9(6) ? N21 C29 H29a . . . 108.9 ? N21 C29 H29b . . . 107.1 ? C28 C29 H29a . . . 110.7 ? C28 C29 H29b . . . 108.4 ? H29a C29 H29b . . . 108.7 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 712 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 10 _reflns_limit_k_min -17 _reflns_limit_k_max 17 _reflns_limit_l_min -17 _reflns_limit_l_max 18 _reflns_number_observed ? _reflns_d_resolution_high .73 _reflns_d_resolution_low 12.174 _diffrn_reflns_av_sigmaI/netI .082 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .082 _refine_ls_wR_factor_all .064 _refine_ls_goodness_of_fit_all 1.594 _refine_ls_shift/su_mean .005 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end data_2 _database_code_CSD 198151 _audit_creation_method Xtal3.6 _audit_creation_date 02-09-09 _audit_update_record ? _chemical_formula_sum 'C15 H37 Br1 Cl2 N6 O11 Zn2' _chemical_formula_moiety [Zn2(T2PrO)Br(H2O)2](ClO4)2 _chemical_formula_weight 755.05 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 11.8040(10) _cell_length_b 10.5204(9) _cell_length_c 21.619(2) _cell_angle_alpha 90.00000 _cell_angle_beta 96.445(2) _cell_angle_gamma 90.00000 _cell_volume 2667.7(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.89 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 22.5 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 3.561 _exptl_crystal_description wedge _exptl_crystal_size_max .2 _exptl_crystal_size_mid .16 _exptl_crystal_size_min .12 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .62 _exptl_absorpt_correction_T_max .86 _diffrn_reflns_number 56052 _reflns_number_total 7023 _reflns_Friedel_coverage 0 _reflns_number_gt 5691 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 28.9 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .054 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .07 _refine_ls_wR_factor_ref .124 _refine_ls_goodness_of_fit_ref 1.289 _refine_ls_number_reflns 5691 _refine_ls_number_parameters 334 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .006 _refine_diff_density_min -1.366 _refine_diff_density_max 4.749 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 60 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 148 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Br ? 0 4 -.374 2.456 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 8 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 24 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 44 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' Zn ? 0 8 .222 1.431 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zn1 .55551(6) .78392(7) .28384(3) .0153(4) Uani ? ? 1.00000 ? ? Zn2 .69901(6) .75364(7) .14164(3) .0172(4) Uani ? ? 1.00000 ? ? Br1 .68520(6) .98677(7) .29201(3) .0250(4) Uani ? ? 1.00000 ? ? O1 .7055(4) .6557(5) .3196(2) .028(2) Uani ? ? 1.00000 ? ? O2 .8274(4) .8232(6) .2056(2) .029(3) Uani ? ? 1.00000 ? ? C11 .4533(6) .5576(6) .2216(3) .020(3) Uani ? ? 1.00000 ? ? N11 .4219(4) .6375(5) .2742(2) .016(2) Uani ? ? 1.00000 ? ? C12 .4365(6) .5733(7) .3348(3) .025(3) Uani ? ? 1.00000 ? ? C13 .4439(7) .6703(7) .3889(3) .026(3) Uani ? ? 1.00000 ? ? N14 .5220(5) .7761(6) .3792(2) .020(3) Uani ? ? 1.00000 ? ? C15 .4752(6) .9029(7) .3904(3) .025(3) Uani ? ? 1.00000 ? ? C16 .3772(6) .9381(7) .3403(3) .025(3) Uani ? ? 1.00000 ? ? N17 .4075(5) .9069(6) .2771(3) .021(3) Uani ? ? 1.00000 ? ? C18 .3178(6) .8378(6) .2388(3) .022(3) Uani ? ? 1.00000 ? ? C19 .3090(5) .7000(7) .2611(3) .020(3) Uani ? ? 1.00000 ? ? C0 .4920(5) .6411(6) .1713(3) .016(3) Uani ? ? 1.00000 ? ? O0 .5820(4) .7229(4) .1981(2) .015(2) Uani ? ? 1.00000 ? ? C21 .5311(5) .5570(6) .1215(3) .018(3) Uani ? ? 1.00000 ? ? N21 .5972(5) .6318(5) .0787(2) .016(2) Uani ? ? 1.00000 ? ? C22 .6770(6) .5565(6) .0468(3) .021(3) Uani ? ? 1.00000 ? ? C23 .7700(6) .6401(7) .0248(3) .024(3) Uani ? ? 1.00000 ? ? N24 .8157(5) .7319(6) .0740(2) .021(3) Uani ? ? 1.00000 ? ? C25 .8240(7) .8649(8) .0510(4) .029(3) Uani ? ? 1.00000 ? ? C26 .7068(7) .9240(7) .0341(4) .029(3) Uani ? ? 1.00000 ? ? N27 .6311(5) .9020(6) .0830(3) .026(3) Uani ? ? 1.00000 ? ? C28 .5164(6) .8520(7) .0593(3) .025(3) Uani ? ? 1.00000 ? ? C29 .5232(6) .7126(7) .0359(3) .022(3) Uani ? ? 1.00000 ? ? Cl1 .46088(14) 1.18839(16) .15165(8) .0233(7) Uani ? ? 1.00000 ? ? O11 .4256(8) 1.0598(6) .1532(4) .062(5) Uani ? ? 1.00000 ? ? O12 .3747(5) 1.2642(7) .1186(4) .046(4) Uani ? ? 1.00000 ? ? O13 .5635(6) 1.1943(9) .1219(4) .065(5) Uani ? ? 1.00000 ? ? O14 .4801(7) 1.2338(9) .2145(4) .063(5) Uani ? ? 1.00000 ? ? Cl2 .16043(19) .7488(2) .04464(9) .0336(9) Uani ? ? 1.00000 ? ? O21 .2127(7) .7439(8) -.0129(3) .054(4) Uani ? ? 1.00000 ? ? O22 .0602(6) .6734(8) .0392(4) .053(4) Uani ? ? 1.00000 ? ? O23 .2414(9) .707(2) .0909(6) .170(13) Uani ? ? 1.00000 ? ? O24 .1284(12) .8787(9) .0494(8) .138(11) Uani ? ? 1.00000 ? ? H11a .38792 .50889 .20514 .02700 Uiso ? ? 1.00000 ? ? H11b .51245 .50016 .23658 .02700 Uiso ? ? 1.00000 ? ? H12a .50318 .52256 .33824 .03200 Uiso ? ? 1.00000 ? ? H12b .37173 .51850 .33782 .03200 Uiso ? ? 1.00000 ? ? H13a .47104 .62523 .42614 .03500 Uiso ? ? 1.00000 ? ? H13b .36988 .70115 .39217 .03500 Uiso ? ? 1.00000 ? ? H14 .58832 .76197 .40507 .02700 Uiso ? ? 1.00000 ? ? H15a .53363 .96384 .39066 .03100 Uiso ? ? 1.00000 ? ? H15b .44632 .90200 .43003 .03100 Uiso ? ? 1.00000 ? ? H16a .36306 1.02719 .34301 .03500 Uiso ? ? 1.00000 ? ? H16b .31071 .89273 .34771 .03500 Uiso ? ? 1.00000 ? ? H17 .43077 .98150 .25000 .02700 Uiso ? ? 1.00000 ? ? H18a .33307 .83813 .19638 .03100 Uiso ? ? 1.00000 ? ? H18b .24612 .87905 .24133 .03100 Uiso ? ? 1.00000 ? ? H19a .27179 .69960 .29712 .02900 Uiso ? ? 1.00000 ? ? H19b .26465 .65343 .22865 .02900 Uiso ? ? 1.00000 ? ? H0 .43146 .69340 .15293 .02100 Uiso ? ? 1.00000 ? ? H21a .46692 .51915 .09749 .02300 Uiso ? ? 1.00000 ? ? H21b .57885 .49083 .14001 .02300 Uiso ? ? 1.00000 ? ? H22a .63643 .51500 .01174 .03000 Uiso ? ? 1.00000 ? ? H22b .71099 .49318 .07462 .03000 Uiso ? ? 1.00000 ? ? H23a .73941 .68664 -.01086 .03300 Uiso ? ? 1.00000 ? ? H23b .83073 .58760 .01401 .03300 Uiso ? ? 1.00000 ? ? H24 .87783 .73334 .08855 .02900 Uiso ? ? 1.00000 ? ? H25a .86467 .86361 .01531 .03800 Uiso ? ? 1.00000 ? ? H25b .86550 .91384 .08283 .03800 Uiso ? ? 1.00000 ? ? H26a .67453 .88875 -.00443 .03800 Uiso ? ? 1.00000 ? ? H26b .71714 1.01335 .02882 .03800 Uiso ? ? 1.00000 ? ? H27 .60579 .99076 .10748 .03200 Uiso ? ? 1.00000 ? ? H28a .48539 .90290 .02486 .03400 Uiso ? ? 1.00000 ? ? H28b .46824 .85399 .09086 .03400 Uiso ? ? 1.00000 ? ? H29a .44810 .67820 .03101 .02700 Uiso ? ? 1.00000 ? ? H29b .55188 .71347 -.00367 .02700 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zn1 .0144(4) .0190(4) .0128(3) -.0016(3) .0029(3) -.0013(2) Zn2 .0157(4) .0225(4) .0143(4) -.0055(3) .0062(3) -.0046(3) Br1 .0258(4) .0235(4) .0265(4) -.0061(3) .0069(3) -.0037(2) O1 .022(3) .033(3) .029(3) .002(2) .001(2) -.001(2) O2 .023(3) .039(3) .024(2) -.007(2) .002(2) -.005(2) C11 .022(3) .018(3) .018(3) -.008(2) .002(2) .000(2) N11 .015(2) .015(2) .020(2) -.003(2) .008(2) -.001(2) C12 .030(4) .030(4) .014(3) -.003(3) .007(3) .004(3) C13 .033(4) .030(4) .016(3) -.004(3) .008(3) .003(3) N14 .016(3) .034(3) .009(2) .001(2) .000(2) .000(2) C15 .025(3) .032(4) .018(3) .001(3) .008(3) -.007(3) C16 .022(3) .030(4) .023(3) .005(3) .003(3) -.007(3) N17 .022(3) .024(3) .018(2) .000(2) .005(2) .001(2) C18 .023(3) .019(3) .023(3) .011(3) -.000(3) -.002(2) C19 .012(3) .024(3) .026(3) -.001(2) .003(2) .002(3) C0 .016(3) .015(3) .016(3) -.004(2) .002(2) -.002(2) O0 .013(2) .023(2) .0107(18) -.0073(17) .0038(16) -.0044(16) C21 .019(3) .018(3) .015(3) .001(2) -.003(2) -.001(2) N21 .018(3) .015(2) .014(2) .001(2) -.000(2) -.0035(18) C22 .029(3) .022(3) .012(3) .005(3) .005(2) -.008(2) C23 .029(4) .027(3) .020(3) .002(3) .013(3) -.003(3) N24 .018(3) .038(3) .010(2) -.004(2) .007(2) -.001(2) C25 .026(4) .035(4) .030(4) -.004(3) .014(3) -.001(3) C26 .031(4) .020(3) .039(4) -.007(3) .009(3) .008(3) N27 .022(3) .020(3) .039(3) -.002(2) .017(3) .003(2) C28 .022(3) .020(3) .033(4) .001(3) .006(3) .009(3) C29 .024(3) .023(3) .017(3) .004(3) .000(2) .009(2) Cl1 .0216(8) .0210(8) .0274(8) .0033(6) .0026(6) .0016(6) O11 .102(7) .018(3) .067(5) -.015(3) .016(5) -.002(3) O12 .021(3) .053(4) .063(4) .010(3) .003(3) .025(3) O13 .036(4) .082(6) .081(6) .013(4) .022(4) .043(5) O14 .046(4) .082(6) .056(5) .021(4) -.020(4) -.041(4) Cl2 .0349(10) .0383(10) .0258(8) -.0135(8) -.0039(7) .0018(7) O21 .045(4) .085(6) .033(3) -.002(4) .013(3) -.011(3) O22 .031(3) .059(5) .065(5) -.015(3) -.002(3) .009(4) O23 .041(5) .36(3) .101(9) -.042(10) -.040(6) .125(13) O24 .164(13) .041(5) .234(17) -.016(7) .136(13) -.036(8) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Zn1 Br1 . . 2.6208(11) ? Zn1 O1 . . 2.289(5) ? Zn1 N11 . . 2.198(5) ? Zn1 N14 . . 2.144(5) ? Zn1 N17 . . 2.166(6) ? Zn1 O0 . . 2.018(4) ? Zn2 O2 . . 2.067(5) ? Zn2 O0 . . 1.971(5) ? Zn2 N21 . . 2.138(5) ? Zn2 N24 . . 2.130(6) ? Zn2 N27 . . 2.112(6) ? C11 N11 . . 1.494(9) ? C11 C0 . . 1.508(9) ? C11 H11a . . .960 ? C11 H11b . . .953 ? N11 C12 . . 1.468(8) ? N11 C19 . . 1.485(8) ? C12 C13 . . 1.546(10) ? C12 H12a . . .947 ? C12 H12b . . .966 ? C13 N14 . . 1.475(10) ? C13 H13a . . .958 ? C13 H13b . . .942 ? N14 C15 . . 1.475(10) ? N14 H14 . . .921 ? C15 C16 . . 1.538(10) ? C15 H15a . . .941 ? C15 H15b . . .957 ? C16 N17 . . 1.487(9) ? C16 H16a . . .955 ? C16 H16b . . .948 ? N17 C18 . . 1.463(9) ? N17 H17 . . 1.034 ? C18 C19 . . 1.535(10) ? C18 H18a . . .954 ? C18 H18b . . .957 ? C19 H19a . . .937 ? C19 H19b . . .961 ? C0 O0 . . 1.438(7) ? C0 C21 . . 1.505(9) ? C0 H0 . . .952 ? C21 N21 . . 1.499(8) ? C21 H21a . . .956 ? C21 H21b . . .955 ? N21 C22 . . 1.462(9) ? N21 C29 . . 1.470(8) ? C22 C23 . . 1.523(10) ? C22 H22a . . .955 ? C22 H22b . . .955 ? C23 N24 . . 1.493(9) ? C23 H23a . . .951 ? C23 H23b . . .954 ? N24 C25 . . 1.492(10) ? N24 H24 . . .764 ? C25 C26 . . 1.524(11) ? C25 H25a . . .954 ? C25 H25b . . .950 ? C26 N27 . . 1.475(11) ? C26 H26a . . .952 ? C26 H26b . . .957 ? N27 C28 . . 1.489(9) ? N27 H27 . . 1.130 ? C28 C29 . . 1.556(10) ? C28 H28a . . .956 ? C28 H28b . . .937 ? C29 H29a . . .953 ? C29 H29b . . .954 ? Cl1 O11 . . 1.417(7) ? Cl1 O12 . . 1.421(7) ? Cl1 O13 . . 1.434(9) ? Cl1 O14 . . 1.435(8) ? Cl2 O21 . . 1.451(8) ? Cl2 O22 . . 1.418(8) ? Cl2 O23 . . 1.375(13) ? Cl2 O24 . . 1.425(11) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Br1 Zn1 O1 . . . 91.92(14) ? Br1 Zn1 N11 . . . 169.97(14) ? Br1 Zn1 N14 . . . 97.81(16) ? Br1 Zn1 N17 . . . 88.77(16) ? Br1 Zn1 O0 . . . 99.87(13) ? O1 Zn1 N11 . . . 97.9(2) ? O1 Zn1 N14 . . . 82.6(2) ? O1 Zn1 N17 . . . 164.1(2) ? O1 Zn1 O0 . . . 85.93(19) ? N11 Zn1 N14 . . . 81.8(2) ? N11 Zn1 N17 . . . 81.2(2) ? N11 Zn1 O0 . . . 82.7(2) ? N14 Zn1 N17 . . . 81.6(2) ? N14 Zn1 O0 . . . 159.2(2) ? N17 Zn1 O0 . . . 109.6(2) ? O2 Zn2 O0 . . . 99.0(2) ? O2 Zn2 N21 . . . 162.8(2) ? O2 Zn2 N24 . . . 90.8(2) ? O2 Zn2 N27 . . . 109.9(2) ? O0 Zn2 N21 . . . 85.0(2) ? O0 Zn2 N24 . . . 163.7(2) ? O0 Zn2 N27 . . . 104.4(2) ? N21 Zn2 N24 . . . 82.0(2) ? N21 Zn2 N27 . . . 85.0(2) ? N24 Zn2 N27 . . . 84.2(2) ? N11 C11 C0 . . . 110.0(5) ? N11 C11 H11a . . . 108.9 ? N11 C11 H11b . . . 109.4 ? C0 C11 H11a . . . 109.9 ? C0 C11 H11b . . . 110.2 ? H11a C11 H11b . . . 108.4 ? Zn1 N11 C11 . . . 103.3(4) ? Zn1 N11 C12 . . . 103.1(4) ? Zn1 N11 C19 . . . 109.1(4) ? C11 N11 C12 . . . 114.0(5) ? C11 N11 C19 . . . 113.4(5) ? C12 N11 C19 . . . 112.8(5) ? N11 C12 C13 . . . 111.3(6) ? N11 C12 H12a . . . 110.0 ? N11 C12 H12b . . . 108.6 ? C13 C12 H12a . . . 109.8 ? C13 C12 H12b . . . 108.7 ? H12a C12 H12b . . . 108.4 ? C12 C13 N14 . . . 111.9(6) ? C12 C13 H13a . . . 107.1 ? C12 C13 H13b . . . 108.1 ? N14 C13 H13a . . . 109.7 ? N14 C13 H13b . . . 110.5 ? H13a C13 H13b . . . 109.5 ? Zn1 N14 C13 . . . 110.6(4) ? Zn1 N14 C15 . . . 103.6(4) ? Zn1 N14 H14 . . . 110.7 ? C13 N14 C15 . . . 114.0(6) ? C13 N14 H14 . . . 107.1 ? C15 N14 H14 . . . 110.8 ? N14 C15 C16 . . . 111.6(6) ? N14 C15 H15a . . . 109.2 ? N14 C15 H15b . . . 108.3 ? C16 C15 H15a . . . 109.5 ? C16 C15 H15b . . . 108.6 ? H15a C15 H15b . . . 109.6 ? C15 C16 N17 . . . 110.8(6) ? C15 C16 H16a . . . 108.4 ? C15 C16 H16b . . . 109.3 ? N17 C16 H16a . . . 109.6 ? N17 C16 H16b . . . 109.5 ? H16a C16 H16b . . . 109.2 ? Zn1 N17 C16 . . . 110.2(4) ? Zn1 N17 C18 . . . 105.6(4) ? Zn1 N17 H17 . . . 103.2 ? C16 N17 C18 . . . 113.3(6) ? C16 N17 H17 . . . 117.3 ? C18 N17 H17 . . . 106.1 ? N17 C18 C19 . . . 111.2(5) ? N17 C18 H18a . . . 109.8 ? N17 C18 H18b . . . 109.3 ? C19 C18 H18a . . . 109.4 ? C19 C18 H18b . . . 108.6 ? H18a C18 H18b . . . 108.5 ? N11 C19 C18 . . . 112.8(5) ? N11 C19 H19a . . . 109.5 ? N11 C19 H19b . . . 108.5 ? C18 C19 H19a . . . 108.6 ? C18 C19 H19b . . . 107.6 ? H19a C19 H19b . . . 109.6 ? C11 C0 O0 . . . 109.1(5) ? C11 C0 C21 . . . 108.3(5) ? C11 C0 H0 . . . 111.3 ? O0 C0 C21 . . . 111.6(5) ? O0 C0 H0 . . . 107.9 ? C21 C0 H0 . . . 108.5 ? Zn1 O0 Zn2 . . . 135.1(2) ? Zn1 O0 C0 . . . 112.2(4) ? Zn2 O0 C0 . . . 112.7(4) ? C0 C21 N21 . . . 110.8(5) ? C0 C21 H21a . . . 110.2 ? C0 C21 H21b . . . 110.1 ? N21 C21 H21a . . . 108.6 ? N21 C21 H21b . . . 108.5 ? H21a C21 H21b . . . 108.6 ? Zn2 N21 C21 . . . 102.5(3) ? Zn2 N21 C22 . . . 106.2(4) ? Zn2 N21 C29 . . . 107.8(4) ? C21 N21 C22 . . . 114.5(5) ? C21 N21 C29 . . . 112.3(5) ? C22 N21 C29 . . . 112.6(5) ? N21 C22 C23 . . . 111.1(6) ? N21 C22 H22a . . . 109.3 ? N21 C22 H22b . . . 109.1 ? C23 C22 H22a . . . 109.4 ? C23 C22 H22b . . . 109.4 ? H22a C22 H22b . . . 108.6 ? C22 C23 N24 . . . 111.6(6) ? C22 C23 H23a . . . 109.2 ? C22 C23 H23b . . . 109.3 ? N24 C23 H23a . . . 108.6 ? N24 C23 H23b . . . 109.1 ? H23a C23 H23b . . . 109.0 ? Zn2 N24 C23 . . . 110.4(4) ? Zn2 N24 C25 . . . 101.5(5) ? Zn2 N24 H24 . . . 112.4 ? C23 N24 C25 . . . 113.7(5) ? C23 N24 H24 . . . 123.9 ? C25 N24 H24 . . . 91.3 ? N24 C25 C26 . . . 111.8(6) ? N24 C25 H25a . . . 108.3 ? N24 C25 H25b . . . 108.3 ? C26 C25 H25a . . . 109.8 ? C26 C25 H25b . . . 109.5 ? H25a C25 H25b . . . 109.2 ? C25 C26 N27 . . . 111.8(6) ? C25 C26 H26a . . . 108.3 ? C25 C26 H26b . . . 107.7 ? N27 C26 H26a . . . 110.6 ? N27 C26 H26b . . . 109.6 ? H26a C26 H26b . . . 108.7 ? Zn2 N27 C26 . . . 109.0(4) ? Zn2 N27 C28 . . . 102.4(4) ? Zn2 N27 H27 . . . 115.5 ? C26 N27 C28 . . . 114.2(6) ? C26 N27 H27 . . . 114.8 ? C28 N27 H27 . . . 100.1 ? N27 C28 C29 . . . 111.5(6) ? N27 C28 H28a . . . 108.9 ? N27 C28 H28b . . . 110.1 ? C29 C28 H28a . . . 107.7 ? C29 C28 H28b . . . 108.4 ? H28a C28 H28b . . . 110.1 ? N21 C29 C28 . . . 112.9(5) ? N21 C29 H29a . . . 109.2 ? N21 C29 H29b . . . 109.0 ? C28 C29 H29a . . . 108.2 ? C28 C29 H29b . . . 108.6 ? H29a C29 H29b . . . 108.9 ? O11 Cl1 O12 . . . 110.6(5) ? O11 Cl1 O13 . . . 108.5(6) ? O11 Cl1 O14 . . . 108.1(5) ? O12 Cl1 O13 . . . 110.1(5) ? O12 Cl1 O14 . . . 108.5(5) ? O13 Cl1 O14 . . . 111.0(5) ? O21 Cl2 O22 . . . 109.9(5) ? O21 Cl2 O23 . . . 106.5(6) ? O21 Cl2 O24 . . . 103.7(8) ? O22 Cl2 O23 . . . 112.8(8) ? O22 Cl2 O24 . . . 108.5(7) ? O23 Cl2 O24 . . . 115.0(11) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1544 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min -29 _reflns_limit_l_max 29 _reflns_number_observed ? _reflns_d_resolution_high .735 _reflns_d_resolution_low 10.795 _diffrn_reflns_av_sigmaI/netI .049 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .086 _refine_ls_wR_factor_all .147 _refine_ls_goodness_of_fit_all 1.373 _refine_ls_shift/su_mean .0003 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end